# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 893758' #TrackingRef 'web_deposit_cif_file_0_TianzhanZhang_1343266833.compound1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16.50 H17.50 N1.50 Na O9.50 V' _chemical_formula_weight 462.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 20.463(4) _cell_length_b 20.463(4) _cell_length_c 27.880(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 10111(3) _cell_formula_units_Z 18 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 20457 _cell_measurement_theta_min 1.36 _cell_measurement_theta_max 27.70 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.368 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4266 _exptl_absorpt_coefficient_mu 0.508 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.881 _exptl_absorpt_correction_T_max 0.894 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean 0.01 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 20457 _diffrn_reflns_av_R_equivalents 0.0653 _diffrn_reflns_av_sigmaI/netI 0.0672 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 27.70 _reflns_number_total 5212 _reflns_number_gt 3559 _reflns_threshold_expression >2sigma(I) _computing_data_collection auto _computing_cell_refinement auto _computing_data_reduction auto _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5212 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.0956 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 0.903 _refine_ls_restrained_S_all 0.903 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.000 636.4 14.4 2 -0.010 0.485 -0.012 3234.6 73.1 3 0.333 0.667 0.667 637.2 14.5 4 0.667 0.333 0.333 637.1 14.5 _platon_squeeze_details ; ? ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.411901(18) 0.098582(18) 0.120184(12) 0.01830(10) Uani 1 1 d . . . Na1 Na 0.39915(5) 0.28033(5) 0.13472(3) 0.0308(2) Uani 1 1 d . . . C1 C 0.24457(12) -0.12733(12) 0.03103(7) 0.0293(5) Uani 1 1 d . . . H1A H 0.2879 -0.1014 0.0125 0.035 Uiso 1 1 calc R . . C2 C 0.30926(11) -0.03094(11) 0.09438(7) 0.0235(4) Uani 1 1 d . . . C3 C 0.11975(12) -0.23163(12) 0.04161(7) 0.0289(5) Uani 1 1 d . . . H3A H 0.0782 -0.2750 0.0298 0.035 Uiso 1 1 calc R . . C4 C 0.18264(11) -0.19122(11) 0.01253(7) 0.0274(5) Uani 1 1 d . . . C5 C 0.24282(11) -0.10159(11) 0.07675(7) 0.0266(5) Uani 1 1 d . . . C6 C 0.58324(11) 0.17007(11) 0.11739(7) 0.0229(4) Uani 1 1 d . . . C7 C 0.58875(11) 0.29575(11) 0.12075(8) 0.0245(5) Uani 1 1 d . . . H7A H 0.5363 0.2703 0.1204 0.029 Uiso 1 1 calc R . . C8 C 0.62643(11) 0.25484(10) 0.12099(8) 0.0234(5) Uani 1 1 d . . . C9 C 0.05044(12) -0.25286(12) 0.11917(7) 0.0273(5) Uani 1 1 d . . . C10 C 0.17916(11) -0.14134(11) 0.10508(7) 0.0279(5) Uani 1 1 d . . . H10A H 0.1772 -0.1235 0.1354 0.033 Uiso 1 1 calc R . . C11 C 0.11823(11) -0.20784(11) 0.08820(7) 0.0261(5) Uani 1 1 d . . . C12 C 0.18459(12) -0.21324(12) -0.03856(7) 0.0270(5) Uani 1 1 d . . . O1 O 0.61340(8) 0.13323(8) 0.12818(6) 0.0351(4) Uani 1 1 d . . . O2 O 0.30009(7) 0.01197(8) 0.12355(5) 0.0260(3) Uani 1 1 d . . . O3 O 0.51607(7) 0.14182(7) 0.09999(5) 0.0259(3) Uani 1 1 d . . . O4 O 0.37403(8) -0.01170(8) 0.07976(5) 0.0274(3) Uani 1 1 d . . . O5 O 0.40076(8) 0.15778(8) 0.15147(5) 0.0290(3) Uani 1 1 d . . . O6 O 0.05621(7) -0.22687(8) 0.16159(5) 0.0281(3) Uani 1 1 d . . . O7 O -0.00501(9) -0.30924(9) 0.10290(6) 0.0487(5) Uani 1 1 d . . . O8 O 0.12235(8) -0.26754(8) -0.05443(5) 0.0300(3) Uani 1 1 d . . . O9 O 0.24333(9) -0.17899(9) -0.06147(5) 0.0400(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.01817(18) 0.01908(18) 0.01671(17) -0.00050(13) -0.00196(13) 0.00861(15) Na1 0.0269(5) 0.0369(5) 0.0315(5) -0.0057(4) -0.0019(4) 0.0181(4) C1 0.0214(11) 0.0296(12) 0.0230(11) -0.0018(9) 0.0072(8) 0.0024(9) C2 0.0248(11) 0.0228(11) 0.0150(10) -0.0006(8) -0.0027(8) 0.0060(9) C3 0.0252(11) 0.0247(11) 0.0234(11) -0.0067(9) 0.0013(9) 0.0025(9) C4 0.0242(11) 0.0255(11) 0.0206(11) -0.0055(8) 0.0048(8) 0.0035(9) C5 0.0208(11) 0.0232(11) 0.0239(11) -0.0039(8) 0.0016(8) 0.0020(9) C6 0.0195(11) 0.0191(10) 0.0285(12) 0.0032(8) 0.0058(8) 0.0082(9) C7 0.0149(10) 0.0200(11) 0.0370(13) -0.0004(9) 0.0015(8) 0.0076(9) C8 0.0190(10) 0.0159(10) 0.0349(12) 0.0005(8) 0.0010(9) 0.0086(8) C9 0.0259(11) 0.0270(12) 0.0212(11) -0.0010(9) 0.0043(9) 0.0073(10) C10 0.0264(11) 0.0278(12) 0.0194(11) -0.0072(8) 0.0029(8) 0.0061(9) C11 0.0234(11) 0.0241(11) 0.0202(11) -0.0020(8) 0.0038(8) 0.0039(9) C12 0.0292(12) 0.0280(12) 0.0183(11) -0.0022(9) 0.0025(9) 0.0102(10) O1 0.0256(8) 0.0213(8) 0.0627(11) 0.0079(7) 0.0037(7) 0.0149(7) O2 0.0195(7) 0.0262(8) 0.0244(8) -0.0065(6) -0.0001(6) 0.0055(6) O3 0.0191(7) 0.0236(8) 0.0297(8) 0.0015(6) 0.0026(6) 0.0068(6) O4 0.0210(8) 0.0257(8) 0.0279(8) -0.0022(6) 0.0023(6) 0.0060(6) O5 0.0330(9) 0.0299(8) 0.0272(8) -0.0041(6) -0.0020(6) 0.0182(7) O6 0.0252(8) 0.0285(8) 0.0216(8) -0.0015(6) 0.0076(6) 0.0066(7) O7 0.0314(9) 0.0445(10) 0.0327(10) -0.0106(8) 0.0111(7) -0.0092(8) O8 0.0262(8) 0.0322(9) 0.0212(8) -0.0085(6) 0.0007(6) 0.0069(7) O9 0.0335(9) 0.0444(10) 0.0220(8) -0.0047(7) 0.0092(7) 0.0044(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 O5 1.5988(14) . ? V1 O3 1.9385(14) . ? V1 O6 1.9836(14) 14 ? V1 O8 2.0048(14) 12 ? V1 O2 2.0808(14) . ? V1 O4 2.2836(14) . ? V1 C2 2.527(2) . ? V1 Na1 3.4097(10) 13 ? Na1 O7 2.3044(17) 2 ? Na1 O9 2.3082(18) 12 ? Na1 O1 2.3433(17) 3_665 ? Na1 O2 2.4678(16) 13 ? Na1 O5 2.5674(17) . ? Na1 O5 2.8131(17) 13 ? Na1 V1 3.4097(10) 13 ? C1 C5 1.386(3) . ? C1 C4 1.387(3) . ? C2 O4 1.247(2) . ? C2 O2 1.278(2) . ? C2 C5 1.488(3) . ? C3 C4 1.391(3) . ? C3 C11 1.393(3) . ? C4 C12 1.500(3) . ? C5 C10 1.387(3) . ? C6 O1 1.227(2) . ? C6 O3 1.290(2) . ? C6 C8 1.506(3) . ? C7 C8 1.379(3) 3_665 ? C7 C8 1.393(3) . ? C8 C7 1.379(3) 2_655 ? C9 O7 1.231(2) . ? C9 O6 1.278(2) . ? C9 C11 1.497(3) . ? C10 C11 1.390(3) . ? C12 O9 1.225(2) . ? C12 O8 1.280(2) . ? O1 Na1 2.3433(17) 2_655 ? O2 Na1 2.4678(16) 13 ? O5 Na1 2.8131(17) 13 ? O6 V1 1.9837(14) 15_445 ? O7 Na1 2.3044(17) 3 ? O8 V1 2.0048(14) 11 ? O9 Na1 2.3082(18) 11 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 V1 O3 110.70(7) . . ? O5 V1 O6 99.67(7) . 14 ? O3 V1 O6 85.02(6) . 14 ? O5 V1 O8 100.41(7) . 12 ? O3 V1 O8 87.29(6) . 12 ? O6 V1 O8 159.92(6) 14 12 ? O5 V1 O2 96.21(6) . . ? O3 V1 O2 153.09(6) . . ? O6 V1 O2 90.61(6) 14 . ? O8 V1 O2 87.89(6) 12 . ? O5 V1 O4 155.71(6) . . ? O3 V1 O4 93.44(5) . . ? O6 V1 O4 84.55(6) 14 . ? O8 V1 O4 77.41(6) 12 . ? O2 V1 O4 59.68(5) . . ? O5 V1 C2 126.25(7) . . ? O3 V1 C2 122.93(6) . . ? O6 V1 C2 88.79(6) 14 . ? O8 V1 C2 79.89(6) 12 . ? O2 V1 C2 30.26(6) . . ? O4 V1 C2 29.50(6) . . ? O5 V1 Na1 54.90(5) . 13 ? O3 V1 Na1 156.33(5) . 13 ? O6 V1 Na1 79.91(4) 14 13 ? O8 V1 Na1 112.57(5) 12 13 ? O2 V1 Na1 45.95(4) . 13 ? O4 V1 Na1 103.10(4) . 13 ? C2 V1 Na1 75.14(5) . 13 ? O7 Na1 O9 92.63(7) 2 12 ? O7 Na1 O1 110.85(7) 2 3_665 ? O9 Na1 O1 86.65(6) 12 3_665 ? O7 Na1 O2 82.77(6) 2 13 ? O9 Na1 O2 175.39(6) 12 13 ? O1 Na1 O2 95.10(6) 3_665 13 ? O7 Na1 O5 132.75(7) 2 . ? O9 Na1 O5 74.66(5) 12 . ? O1 Na1 O5 113.48(6) 3_665 . ? O2 Na1 O5 108.40(6) 13 . ? O7 Na1 O5 76.65(6) 2 13 ? O9 Na1 O5 116.31(6) 12 13 ? O1 Na1 O5 156.04(6) 3_665 13 ? O2 Na1 O5 62.56(5) 13 13 ? O5 Na1 O5 69.60(5) . 13 ? O7 Na1 V1 68.30(5) 2 13 ? O9 Na1 V1 140.33(5) 12 13 ? O1 Na1 V1 132.13(5) 3_665 13 ? O2 Na1 V1 37.30(3) 13 13 ? O5 Na1 V1 92.79(4) . 13 ? O5 Na1 V1 27.71(3) 13 13 ? C5 C1 C4 120.99(19) . . ? O4 C2 O2 119.27(18) . . ? O4 C2 C5 120.61(18) . . ? O2 C2 C5 120.08(18) . . ? O4 C2 V1 64.36(10) . . ? O2 C2 V1 55.15(9) . . ? C5 C2 V1 171.65(15) . . ? C4 C3 C11 120.78(19) . . ? C1 C4 C3 118.78(19) . . ? C1 C4 C12 119.15(18) . . ? C3 C4 C12 122.05(18) . . ? C1 C5 C10 119.73(18) . . ? C1 C5 C2 119.22(18) . . ? C10 C5 C2 121.04(18) . . ? O1 C6 O3 124.58(18) . . ? O1 C6 C8 120.38(18) . . ? O3 C6 C8 114.93(17) . . ? C8 C7 C8 120.72(19) 3_665 . ? C7 C8 C7 119.28(19) 2_655 . ? C7 C8 C6 119.90(17) 2_655 . ? C7 C8 C6 120.63(18) . . ? O7 C9 O6 125.53(19) . . ? O7 C9 C11 120.05(18) . . ? O6 C9 C11 114.41(18) . . ? C5 C10 C11 120.08(19) . . ? C10 C11 C3 119.48(18) . . ? C10 C11 C9 120.60(18) . . ? C3 C11 C9 119.90(18) . . ? O9 C12 O8 125.6(2) . . ? O9 C12 C4 119.27(19) . . ? O8 C12 C4 115.13(17) . . ? C6 O1 Na1 151.66(14) . 2_655 ? C2 O2 V1 94.59(11) . . ? C2 O2 Na1 158.62(13) . 13 ? V1 O2 Na1 96.75(5) . 13 ? C6 O3 V1 141.02(13) . . ? C2 O4 V1 86.14(12) . . ? V1 O5 Na1 135.82(8) . . ? V1 O5 Na1 97.38(6) . 13 ? Na1 O5 Na1 110.40(5) . 13 ? C9 O6 V1 130.94(13) . 15_445 ? C9 O7 Na1 134.15(14) . 3 ? C12 O8 V1 128.73(13) . 11 ? C12 O9 Na1 137.11(16) . 11 ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.70 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.328 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.061 data_3 _database_code_depnum_ccdc_archive 'CCDC 893759' #TrackingRef 'compound 2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H42 Li N3 O13 V' _chemical_formula_weight 710.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 18.079(4) _cell_length_b 16.435(3) _cell_length_c 11.603(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3447.6(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 28417 _cell_measurement_theta_min 3.11 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1492 _exptl_absorpt_coefficient_mu 0.354 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9554 _exptl_absorpt_correction_T_max 0.9790 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March,1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean 0.01 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 28417 _diffrn_reflns_av_R_equivalents 0.1046 _diffrn_reflns_av_sigmaI/netI 0.0991 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7671 _reflns_number_gt 4991 _reflns_threshold_expression >2sigma(I) _computing_data_collection auto _computing_cell_refinement auto _computing_data_reduction auto _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0678P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.06(3) _refine_ls_number_reflns 7671 _refine_ls_number_parameters 433 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.1045 _refine_ls_R_factor_gt 0.0609 _refine_ls_wR_factor_ref 0.1480 _refine_ls_wR_factor_gt 0.1293 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.30264(3) 0.08712(4) 0.62800(6) 0.02076(15) Uani 1 1 d . . . Li1 Li 0.2262(5) 0.1026(5) 0.8606(7) 0.039(2) Uani 1 1 d . . . O1 O 0.3038(2) 0.0859(2) 0.4209(3) 0.0397(8) Uani 1 1 d . . . O2 O 0.30015(17) -0.02063(17) 0.5326(2) 0.0281(6) Uani 1 1 d . . . O3 O 0.30007(17) 0.04415(18) 0.7516(2) 0.0293(7) Uani 1 1 d . . . O4 O 0.20176(19) -0.29463(19) 0.1665(2) 0.0328(7) Uani 1 1 d . . . O5 O 0.40865(17) 0.10413(19) 0.5985(2) 0.0327(8) Uani 1 1 d . . . O6 O 0.2214(2) 0.0737(2) 0.0194(3) 0.0441(9) Uani 1 1 d . . . O7 O 0.1912(3) -0.0443(3) -0.0598(3) 0.0595(12) Uani 1 1 d . . . O8 O 0.4622(2) 0.1446(3) 0.7617(3) 0.0547(11) Uani 1 1 d . . . O9 O 0.2247(2) -0.2901(2) 0.3566(3) 0.0411(9) Uani 1 1 d . . . O10 O 0.64580(19) 0.3680(2) 0.7545(3) 0.0475(10) Uani 1 1 d . . . O11 O 0.69638(17) 0.3993(2) 0.5856(3) 0.0366(8) Uani 1 1 d . . . O12 O 0.5321(3) 0.3621(3) 0.2409(4) 0.0829(17) Uani 1 1 d . . . O13 O 0.4681(3) 0.2486(3) 0.2315(3) 0.0649(13) Uani 1 1 d . . . C1 C 0.2928(2) 0.0121(3) 0.4338(4) 0.0275(9) Uani 1 1 d . . . C2 C 0.2672(2) -0.0401(3) 0.3340(4) 0.0233(9) Uani 1 1 d . . . C3 C 0.2513(3) -0.0005(3) 0.2305(4) 0.0294(10) Uani 1 1 d . . . H3A H 0.2589 0.0553 0.2241 0.035 Uiso 1 1 calc R . . C4 C 0.2240(2) -0.0443(3) 0.1364(4) 0.0274(9) Uani 1 1 d . . . C5 C 0.2131(2) -0.1273(3) 0.1477(4) 0.0305(10) Uani 1 1 d . . . H5A H 0.1951 -0.1568 0.0853 0.037 Uiso 1 1 calc R . . C6 C 0.2284(2) -0.1676(3) 0.2505(4) 0.0257(9) Uani 1 1 d . . . C7 C 0.2566(2) -0.1230(3) 0.3428(4) 0.0248(9) Uani 1 1 d . . . H7A H 0.2683 -0.1495 0.4112 0.030 Uiso 1 1 calc R . . C8 C 0.2114(2) -0.0019(3) 0.0218(4) 0.0328(10) Uani 1 1 d . . . C9 C 0.4805(2) 0.2256(3) 0.4726(4) 0.0274(10) Uani 1 1 d . . . H9A H 0.4447 0.1948 0.4351 0.033 Uiso 1 1 calc R . . C10 C 0.5399(4) 0.5579(5) 0.3227(6) 0.078(2) Uani 1 1 d . . . H10A H 0.5795 0.5906 0.2928 0.117 Uiso 1 1 calc R . . H10B H 0.4966 0.5653 0.2759 0.117 Uiso 1 1 calc R . . H10C H 0.5542 0.5017 0.3216 0.117 Uiso 1 1 calc R . . C11 C 0.6472(2) 0.3655(3) 0.6475(4) 0.0298(10) Uani 1 1 d . . . C12 C 0.5481(2) 0.2594(3) 0.6451(4) 0.0287(10) Uani 1 1 d . . . H12A H 0.5565 0.2516 0.7234 0.034 Uiso 1 1 calc R . . C13 C 0.4518(2) 0.1506(3) 0.6578(4) 0.0301(10) Uani 1 1 d . . . C14 C 0.1735(4) 0.3522(5) 0.2960(8) 0.095(3) Uani 1 1 d . . . H14A H 0.1349 0.3199 0.3296 0.142 Uiso 1 1 calc R . . H14B H 0.1540 0.3824 0.2320 0.142 Uiso 1 1 calc R . . H14C H 0.1925 0.3893 0.3527 0.142 Uiso 1 1 calc R . . C15 C 0.5856(5) 0.5662(6) 0.5203(9) 0.108(3) Uani 1 1 d U . . H15A H 0.6273 0.5988 0.4979 0.162 Uiso 1 1 calc R . . H15B H 0.5985 0.5097 0.5152 0.162 Uiso 1 1 calc R . . H15C H 0.5720 0.5790 0.5982 0.162 Uiso 1 1 calc R . . C16 C 0.2029(5) 0.2409(7) 0.1695(9) 0.129(4) Uani 1 1 d . . . H16A H 0.1649 0.2084 0.2044 0.194 Uiso 1 1 calc R . . H16B H 0.2420 0.2062 0.1425 0.194 Uiso 1 1 calc R . . H16C H 0.1826 0.2706 0.1057 0.194 Uiso 1 1 calc R . . C17 C 0.2927(4) 0.3509(4) 0.2041(6) 0.0691(19) Uani 1 1 d . . . H17A H 0.3327 0.3169 0.1787 0.104 Uiso 1 1 calc R . . H17B H 0.3106 0.3886 0.2608 0.104 Uiso 1 1 calc R . . H17C H 0.2730 0.3804 0.1395 0.104 Uiso 1 1 calc R . . C18 C 0.2175(2) -0.2575(3) 0.2608(4) 0.0279(10) Uani 1 1 d . . . C19 C 0.5196(3) 0.2853(3) 0.4122(4) 0.0292(10) Uani 1 1 d . . . C20 C 0.4951(2) 0.2123(3) 0.5887(4) 0.0271(9) Uani 1 1 d . . . C21 C 0.5051(3) 0.2996(4) 0.2836(4) 0.0408(13) Uani 1 1 d . . . C22 C 0.4992(7) 0.6654(6) 0.4511(8) 0.119(3) Uani 1 1 d U . . H22A H 0.5379 0.7008 0.4251 0.178 Uiso 1 1 calc R . . H22B H 0.4870 0.6781 0.5296 0.178 Uiso 1 1 calc R . . H22C H 0.4562 0.6728 0.4035 0.178 Uiso 1 1 calc R . . C23 C 0.4630(5) 0.5342(8) 0.4853(9) 0.133(4) Uani 1 1 d . . . H23A H 0.4510 0.5501 0.5627 0.199 Uiso 1 1 calc R . . H23B H 0.4772 0.4779 0.4845 0.199 Uiso 1 1 calc R . . H23C H 0.4207 0.5418 0.4366 0.199 Uiso 1 1 calc R . . C24 C 0.1037(3) 0.6345(3) 0.5320(5) 0.0499(13) Uani 1 1 d . . . H24A H 0.1050 0.6497 0.4522 0.075 Uiso 1 1 calc R . . H24B H 0.1508 0.6124 0.5540 0.075 Uiso 1 1 calc R . . H24C H 0.0932 0.6816 0.5781 0.075 Uiso 1 1 calc R . . C25 C -0.0274(3) 0.6071(4) 0.5205(6) 0.0626(17) Uani 1 1 d . . . H25A H -0.0282 0.6208 0.4400 0.094 Uiso 1 1 calc R . . H25B H -0.0359 0.6553 0.5654 0.094 Uiso 1 1 calc R . . H25C H -0.0654 0.5680 0.5365 0.094 Uiso 1 1 calc R . . C26 C 0.0450(4) 0.5498(5) 0.6760(5) 0.0628(18) Uani 1 1 d . . . H26A H 0.0077 0.5093 0.6897 0.094 Uiso 1 1 calc R . . H26B H 0.0345 0.5972 0.7215 0.094 Uiso 1 1 calc R . . H26C H 0.0926 0.5285 0.6969 0.094 Uiso 1 1 calc R . . C27 C 0.0624(5) 0.5010(4) 0.4788(6) 0.081(2) Uani 1 1 d . . . H27A H 0.0615 0.5162 0.3989 0.121 Uiso 1 1 calc R . . H27B H 0.0262 0.4593 0.4923 0.121 Uiso 1 1 calc R . . H27C H 0.1106 0.4809 0.4984 0.121 Uiso 1 1 calc R . . C28 C 0.2643(6) 0.2538(6) 0.3519(7) 0.114(3) Uani 1 1 d . . . H28A H 0.2266 0.2204 0.3861 0.170 Uiso 1 1 calc R . . H28B H 0.2830 0.2911 0.4084 0.170 Uiso 1 1 calc R . . H28C H 0.3038 0.2199 0.3245 0.170 Uiso 1 1 calc R . . C29 C 0.5882(2) 0.3174(3) 0.5861(4) 0.0275(10) Uani 1 1 d . . . C30 C 0.5741(3) 0.3299(3) 0.4687(4) 0.0320(10) Uani 1 1 d . . . H30A H 0.6014 0.3684 0.4281 0.038 Uiso 1 1 calc R . . N1 N 0.5233(3) 0.5831(3) 0.4436(4) 0.0468(11) Uani 1 1 d . . . N2 N 0.2330(3) 0.2990(3) 0.2561(4) 0.0493(11) Uani 1 1 d . . . N3 N 0.0451(3) 0.5724(3) 0.5503(4) 0.0414(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0252(3) 0.0148(3) 0.0223(3) -0.0014(3) -0.0007(4) 0.0010(3) Li1 0.046(5) 0.039(5) 0.033(4) 0.012(3) 0.001(4) 0.004(4) O1 0.056(2) 0.0207(16) 0.0428(18) -0.0050(15) -0.0091(18) -0.0065(16) O2 0.0373(16) 0.0232(15) 0.0238(14) -0.0052(13) -0.0030(15) 0.0018(13) O3 0.0365(17) 0.0225(17) 0.0290(15) 0.0019(13) -0.0005(14) 0.0010(14) O4 0.0497(18) 0.0198(16) 0.0289(15) -0.0052(12) -0.0001(15) -0.0063(15) O5 0.0316(16) 0.0326(19) 0.0339(18) -0.0083(13) 0.0036(14) -0.0077(13) O6 0.061(2) 0.036(2) 0.0350(17) 0.0175(16) -0.0075(19) -0.0068(16) O7 0.096(3) 0.051(3) 0.0316(18) -0.0052(18) -0.021(2) 0.006(2) O8 0.065(3) 0.070(3) 0.0294(18) 0.0116(18) -0.0082(18) -0.037(2) O9 0.073(3) 0.0214(17) 0.0290(17) 0.0037(14) -0.0019(17) -0.0013(16) O10 0.042(2) 0.066(3) 0.0349(18) -0.0089(18) -0.0040(16) -0.0250(18) O11 0.0279(16) 0.043(2) 0.0390(16) 0.0107(14) -0.0067(14) -0.0124(16) O12 0.125(4) 0.083(4) 0.041(2) 0.024(2) -0.016(3) -0.050(3) O13 0.103(4) 0.063(3) 0.0284(18) -0.0029(19) -0.021(2) -0.022(3) C1 0.027(2) 0.022(2) 0.034(2) -0.0026(18) 0.001(2) 0.0009(18) C2 0.025(2) 0.021(2) 0.023(2) -0.0002(18) 0.0064(18) -0.0012(17) C3 0.040(3) 0.018(2) 0.030(2) 0.0018(18) 0.006(2) -0.004(2) C4 0.036(2) 0.026(2) 0.021(2) 0.000(2) -0.003(2) 0.0000(16) C5 0.041(3) 0.029(2) 0.021(2) -0.0061(19) 0.000(2) -0.0016(18) C6 0.032(2) 0.017(2) 0.028(2) -0.0029(18) 0.006(2) 0.0008(18) C7 0.036(2) 0.017(2) 0.022(2) -0.0006(18) 0.0032(19) -0.0019(18) C8 0.034(3) 0.040(3) 0.024(2) 0.006(2) -0.002(2) 0.001(2) C9 0.024(2) 0.026(2) 0.032(2) -0.0067(18) -0.0037(19) -0.0042(18) C10 0.089(5) 0.093(6) 0.053(4) -0.016(4) 0.008(4) -0.004(4) C11 0.028(2) 0.030(2) 0.031(3) 0.0036(19) -0.009(2) -0.0065(18) C12 0.0256(19) 0.038(2) 0.023(2) -0.0016(19) 0.000(2) -0.0046(17) C13 0.032(2) 0.028(2) 0.030(2) -0.0010(18) -0.0041(19) -0.0018(19) C14 0.063(4) 0.059(5) 0.163(9) -0.022(5) 0.024(5) 0.007(4) C15 0.094(4) 0.129(5) 0.100(4) -0.008(4) -0.018(4) 0.018(4) C16 0.116(8) 0.128(9) 0.144(10) -0.087(7) 0.001(7) -0.023(7) C17 0.078(5) 0.060(5) 0.070(4) -0.004(3) 0.013(4) -0.003(4) C18 0.033(3) 0.021(2) 0.029(2) -0.0001(19) 0.0036(19) 0.0015(18) C19 0.033(2) 0.029(2) 0.025(2) -0.0015(18) -0.001(2) 0.002(2) C20 0.023(2) 0.031(2) 0.028(2) -0.0018(18) 0.0002(18) -0.0007(18) C21 0.045(3) 0.051(4) 0.026(2) 0.000(2) -0.007(2) 0.000(3) C22 0.154(5) 0.112(5) 0.090(4) -0.006(4) -0.009(4) 0.013(4) C23 0.091(7) 0.193(12) 0.113(8) -0.004(8) 0.023(6) -0.049(7) C24 0.044(3) 0.050(3) 0.055(3) -0.003(3) 0.012(3) -0.003(2) C25 0.041(3) 0.098(5) 0.050(3) 0.003(4) 0.009(3) -0.006(3) C26 0.079(5) 0.069(5) 0.040(3) 0.008(3) 0.004(3) 0.003(4) C27 0.130(7) 0.044(4) 0.068(4) -0.018(3) 0.026(4) -0.014(4) C28 0.177(10) 0.078(6) 0.086(6) 0.044(5) -0.018(6) 0.009(6) C29 0.023(2) 0.031(3) 0.028(2) -0.0004(18) -0.0048(18) -0.0031(19) C30 0.039(3) 0.029(2) 0.028(2) 0.0016(19) 0.006(2) -0.007(2) N1 0.044(3) 0.050(3) 0.046(2) -0.004(2) 0.004(2) 0.002(2) N2 0.053(3) 0.035(3) 0.060(3) 0.001(2) 0.007(2) 0.005(2) N3 0.048(3) 0.037(3) 0.039(2) 0.0010(19) 0.003(2) -0.0049(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 O3 1.600(3) . ? V1 O5 1.967(3) . ? V1 O11 1.996(3) 4_455 ? V1 O4 1.996(3) 3 ? V1 O2 2.089(3) . ? V1 O1 2.404(3) . ? V1 C1 2.574(5) . ? V1 Li1 3.043(8) . ? Li1 O6 1.904(8) 1_556 ? Li1 O10 1.965(9) 4_455 ? Li1 O9 1.976(9) 3 ? Li1 O3 2.075(9) . ? Li1 C8 2.553(9) 1_556 ? Li1 O7 2.661(9) 1_556 ? Li1 C18 2.769(10) 3 ? O1 C1 1.238(5) . ? O2 C1 1.273(5) . ? O4 C18 1.285(5) . ? O4 V1 1.996(3) 3_544 ? O5 C13 1.290(5) . ? O6 C8 1.256(6) . ? O6 Li1 1.904(8) 1_554 ? O7 C8 1.231(6) . ? O7 Li1 2.661(9) 1_554 ? O8 C13 1.224(5) . ? O9 C18 1.240(5) . ? O9 Li1 1.976(9) 3_544 ? O10 C11 1.242(5) . ? O10 Li1 1.965(9) 4 ? O11 C11 1.272(5) . ? O11 V1 1.996(3) 4 ? O12 C21 1.240(7) . ? O13 C21 1.230(6) . ? C1 C2 1.514(6) . ? C2 C7 1.379(6) . ? C2 C3 1.397(6) . ? C3 C4 1.398(6) . ? C3 H3A 0.9300 . ? C4 C5 1.385(6) . ? C4 C8 1.518(6) . ? C5 C6 1.391(6) . ? C5 H5A 0.9300 . ? C6 C7 1.394(6) . ? C6 C18 1.497(6) . ? C7 H7A 0.9300 . ? C8 Li1 2.553(9) 1_554 ? C9 C20 1.391(6) . ? C9 C19 1.397(6) . ? C9 H9A 0.9300 . ? C10 N1 1.493(8) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C29 1.506(6) . ? C12 C29 1.379(6) . ? C12 C20 1.395(6) . ? C12 H12A 0.9300 . ? C13 C20 1.512(6) . ? C14 N2 1.462(8) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 N1 1.462(9) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 N2 1.489(9) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 N2 1.502(8) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 Li1 2.769(10) 3_544 ? C19 C30 1.392(6) . ? C19 C21 1.534(6) . ? C22 N1 1.425(10) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 N1 1.439(9) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 N3 1.486(6) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 N3 1.471(7) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 N3 1.505(6) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 N3 1.472(7) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 N2 1.452(8) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.401(6) . ? C30 H30A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 V1 O5 104.30(14) . . ? O3 V1 O11 104.03(15) . 4_455 ? O5 V1 O11 151.56(13) . 4_455 ? O3 V1 O4 103.18(14) . 3 ? O5 V1 O4 86.52(13) . 3 ? O11 V1 O4 84.72(14) 4_455 3 ? O3 V1 O2 95.75(14) . . ? O5 V1 O2 92.83(12) . . ? O11 V1 O2 86.75(12) 4_455 . ? O4 V1 O2 160.63(12) 3 . ? O3 V1 O1 153.30(14) . . ? O5 V1 O1 79.56(12) . . ? O11 V1 O1 76.28(13) 4_455 . ? O4 V1 O1 103.43(12) 3 . ? O2 V1 O1 57.54(12) . . ? O3 V1 C1 124.86(15) . . ? O5 V1 C1 89.04(13) . . ? O11 V1 C1 76.77(13) 4_455 . ? O4 V1 C1 131.25(13) 3 . ? O2 V1 C1 29.41(12) . . ? O1 V1 C1 28.53(12) . . ? O3 V1 Li1 39.48(19) . . ? O5 V1 Li1 125.80(19) . . ? O11 V1 Li1 76.83(19) 4_455 . ? O4 V1 Li1 72.67(19) 3 . ? O2 V1 Li1 122.06(19) . . ? O1 V1 Li1 153.07(19) . . ? C1 V1 Li1 141.7(2) . . ? O6 Li1 O10 129.4(5) 1_556 4_455 ? O6 Li1 O9 105.4(4) 1_556 3 ? O10 Li1 O9 95.6(4) 4_455 3 ? O6 Li1 O3 120.2(4) 1_556 . ? O10 Li1 O3 102.0(4) 4_455 . ? O9 Li1 O3 96.3(4) 3 . ? O6 Li1 C8 28.23(19) 1_556 1_556 ? O10 Li1 C8 123.2(4) 4_455 1_556 ? O9 Li1 C8 131.7(4) 3 1_556 ? O3 Li1 C8 101.7(4) . 1_556 ? O6 Li1 O7 55.1(2) 1_556 1_556 ? O10 Li1 O7 105.4(4) 4_455 1_556 ? O9 Li1 O7 157.7(4) 3 1_556 ? O3 Li1 O7 86.9(3) . 1_556 ? C8 Li1 O7 27.20(16) 1_556 1_556 ? O6 Li1 C18 128.9(4) 1_556 3 ? O10 Li1 C18 78.8(3) 4_455 3 ? O9 Li1 C18 23.53(16) 3 3 ? O3 Li1 C18 83.8(3) . 3 ? C8 Li1 C18 154.6(4) 1_556 3 ? O7 Li1 C18 170.4(4) 1_556 3 ? O6 Li1 V1 149.1(4) 1_556 . ? O10 Li1 V1 78.5(3) 4_455 . ? O9 Li1 V1 81.3(3) 3 . ? O3 Li1 V1 29.35(14) . . ? C8 Li1 V1 129.9(4) 1_556 . ? O7 Li1 V1 109.9(3) 1_556 . ? C18 Li1 V1 62.04(19) 3 . ? C1 O1 V1 83.4(3) . . ? C1 O2 V1 96.9(3) . . ? V1 O3 Li1 111.2(3) . . ? C18 O4 V1 131.4(3) . 3_544 ? C13 O5 V1 125.5(3) . . ? C8 O6 Li1 106.0(4) . 1_554 ? C8 O7 Li1 71.5(3) . 1_554 ? C18 O9 Li1 116.9(4) . 3_544 ? C11 O10 Li1 128.3(4) . 4 ? C11 O11 V1 125.6(3) . 4 ? O1 C1 O2 120.5(4) . . ? O1 C1 C2 120.8(4) . . ? O2 C1 C2 118.7(4) . . ? O1 C1 V1 68.1(3) . . ? O2 C1 V1 53.7(2) . . ? C2 C1 V1 164.2(3) . . ? C7 C2 C3 119.7(4) . . ? C7 C2 C1 123.1(4) . . ? C3 C2 C1 117.1(4) . . ? C2 C3 C4 120.2(4) . . ? C2 C3 H3A 119.9 . . ? C4 C3 H3A 119.9 . . ? C5 C4 C3 119.0(4) . . ? C5 C4 C8 120.9(4) . . ? C3 C4 C8 120.0(4) . . ? C4 C5 C6 121.4(4) . . ? C4 C5 H5A 119.3 . . ? C6 C5 H5A 119.3 . . ? C5 C6 C7 118.8(4) . . ? C5 C6 C18 120.8(4) . . ? C7 C6 C18 120.4(4) . . ? C2 C7 C6 120.9(4) . . ? C2 C7 H7A 119.5 . . ? C6 C7 H7A 119.5 . . ? O7 C8 O6 125.8(5) . . ? O7 C8 C4 117.3(4) . . ? O6 C8 C4 116.9(4) . . ? O7 C8 Li1 81.3(4) . 1_554 ? O6 C8 Li1 45.8(3) . 1_554 ? C4 C8 Li1 159.1(4) . 1_554 ? C20 C9 C19 120.0(4) . . ? C20 C9 H9A 120.0 . . ? C19 C9 H9A 120.0 . . ? N1 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O10 C11 O11 124.3(4) . . ? O10 C11 C29 118.5(4) . . ? O11 C11 C29 117.2(4) . . ? C29 C12 C20 120.8(4) . . ? C29 C12 H12A 119.6 . . ? C20 C12 H12A 119.6 . . ? O8 C13 O5 124.8(4) . . ? O8 C13 C20 119.7(4) . . ? O5 C13 C20 115.4(4) . . ? N2 C14 H14A 109.5 . . ? N2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 H15A 109.5 . . ? N1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 C16 H16A 109.5 . . ? N2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O9 C18 O4 125.6(4) . . ? O9 C18 C6 118.9(4) . . ? O4 C18 C6 115.5(4) . . ? O9 C18 Li1 39.5(3) . 3_544 ? O4 C18 Li1 92.5(3) . 3_544 ? C6 C18 Li1 143.6(4) . 3_544 ? C30 C19 C9 119.5(4) . . ? C30 C19 C21 119.9(4) . . ? C9 C19 C21 120.6(4) . . ? C9 C20 C12 119.9(4) . . ? C9 C20 C13 121.4(4) . . ? C12 C20 C13 118.7(4) . . ? O13 C21 O12 125.6(5) . . ? O13 C21 C19 117.8(5) . . ? O12 C21 C19 116.6(5) . . ? N1 C22 H22A 109.5 . . ? N1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N1 C23 H23A 109.5 . . ? N1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N3 C24 H24A 109.5 . . ? N3 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N3 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N3 C25 H25A 109.5 . . ? N3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N3 C26 H26A 109.5 . . ? N3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N3 C27 H27A 109.5 . . ? N3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N2 C28 H28A 109.5 . . ? N2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C12 C29 C30 119.3(4) . . ? C12 C29 C11 120.0(4) . . ? C30 C29 C11 120.8(4) . . ? C19 C30 C29 120.6(4) . . ? C19 C30 H30A 119.7 . . ? C29 C30 H30A 119.7 . . ? C22 N1 C23 106.1(8) . . ? C22 N1 C15 112.3(6) . . ? C23 N1 C15 105.8(7) . . ? C22 N1 C10 112.4(6) . . ? C23 N1 C10 108.3(6) . . ? C15 N1 C10 111.4(6) . . ? C28 N2 C14 110.5(7) . . ? C28 N2 C16 109.3(7) . . ? C14 N2 C16 109.2(6) . . ? C28 N2 C17 108.6(6) . . ? C14 N2 C17 108.5(5) . . ? C16 N2 C17 110.8(6) . . ? C25 N3 C27 111.4(5) . . ? C25 N3 C24 109.6(4) . . ? C27 N3 C24 108.5(5) . . ? C25 N3 C26 108.8(5) . . ? C27 N3 C26 110.5(5) . . ? C24 N3 C26 108.0(5) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.551 _refine_diff_density_min -0.430 _refine_diff_density_rms 0.065